Title of Invention	METHOD FOR CURING/DRYING STARCHES RICH IN AMYLOSE
Abstract	The invention concerns a method for preparing pre-gelatinized starch rich in amylose characterised in that it comprises steps which consist in: forming a suspension comprising a starch rich in amylose and water; subjecting said suspension to a vapour jet cooking at a temperature ranging between 125 and 135°C so as to obtain a starch glue rich in pre-gelatinized amylose; cooking and drying said pre-gelatinized starch glue on a drying drum at a pressure ranging between 2 and 10 bars so as to obtain a pre-gelatinized starch rich in amylose. The invention also concerns a pre-gelatinized starch rich in amylose characterised in that it has an apparent density less than 0.4g/ml for an average grain size distribution of 100 micrometers. The invention further concerns such a starch for making soft capsules or tablets and film-coating of solid pharmaceutical, food or agricultural formulations.

Title of Invention

METHOD FOR CURING/DRYING STARCHES RICH IN AMYLOSE

Abstract

The invention concerns a method for preparing pre-gelatinized starch rich in amylose characterised in that it comprises steps which consist in: forming a suspension comprising a starch rich in amylose and water; subjecting said suspension to a vapour jet cooking at a temperature ranging between 125 and 135°C so as to obtain a starch glue rich in pre-gelatinized amylose; cooking and drying said pre-gelatinized starch glue on a drying drum at a pressure ranging between 2 and 10 bars so as to obtain a pre-gelatinized starch rich in amylose. The invention also concerns a pre-gelatinized starch rich in amylose characterised in that it has an apparent density less than 0.4g/ml for an average grain size distribution of 100 micrometers. The invention further concerns such a starch for making soft capsules or tablets and film-coating of solid pharmaceutical, food or agricultural formulations.

Full Text	The subject of the invention is a novel process for preparing pregelatinized amylose-rich starches. Its subject is also the starches obtained by this process. Pregelatinized starches are generally prepared by thermal, chemical or mechanical techniques which can cause swelling of the starch granules so that they are soluble in cold water. The preferred techniques are spray-drying, cooking on a drum or extrusion. Autoclaving or indirect heating on a heat exchanger are cooking processes which tend to produce complex colloidal dispersions consisting of intact, fragmented and swollen granules. It is well known that amylose-rich starches, that is to say which have more than 50% by weight of amylose, are particularly difficult to disperse and require high cooking temperatures. The document US-A-3 086 890 describes a process for preparing pregelatinized amylose. This process consists in autoclaving at 191°C, under pressure, a solution of amylose containing at most 25% by weight of dry matter, and then drum-drying at 110-200°C. The powders obtained are amorphous and form irreversible gels after dispersion. Their apparent density is high, that is to say generally greater than 0.4 g/ml. The document US-A-3 607 394 describes a process for the pregelatinization of starches having amylose contents of less than 60% by weight. This process consists in cooking the starch at 149°C, followed by drum-drying, spray-drying or another type of drying means. The document EP 0 366 898 describes a coupled cooking/ spray-drying process which makes it possible to obtain amorphous products, which are practically free of retrogradation, and which have an apparent density greater than that of an identical starch which has been subjected to the same process but in two separate stages, that is an apparent density greater than 0.45 g/ml. The cooking of amylose-rich starches is carried out on a jet cooker at 143°C and the spray- drying is carried out with an inlet air temperature of 220°C. This document presents, in Figure 7, a comparison of various prior art pregelatinized starches. Starting from this teaching, the applicant has now found, after long research studies, that it was possible to prepare a pregelatinized amylose-rich starch using a particular process leading to products of low apparent density while working at not very high temperatures, which none of the prior art techniques made it possible to obtain. The subject of the invention is therefore a process for preparing pregelatinized amylose-rich starch, characterized in that it comprises the steps consisting in: forming a suspension comprising an amylose-rich starch and water; subjecting the said suspension to steam jet cooking at a temperature of between 125 and 135°C so as to obtain a pregelatinized amylose- rich starch paste; - drying the said pregelatinized starch on a drum dryer at a pressure of between 2 and 10 bar, so as to obtain a pregelatinized amylose-rich starch. The pregelatinized amylose-rich starch obtained may then be recovered and ground so as to obtain a powder having a particle size which is chosen according to the uses which will be subsequently made thereof. The expression "amylose-rich starches" according for the purposes of the present invention denotes starches having an amylose content greater than or equal to 50% by weight, and preferably of between 50 and 80% by weight, obtained from any plant origin, such as in particular maize, potato, cassava. Preferably, the process according to the invention uses a maize starch such as, for example, EURYLON® marketed by the applicant. The invention also applies to chemically or physically modified amylose-rich starches. Preferably, the modified starch will be chosen from the group consisting of acetylated, hydroxypropylated, carboxy- methylated and fluidified starches, and starch octenyl succinates. According to a preferred variant of the process according to the invention, an acetylated starch will be chosen. The starch suspension is prepared at a dry matter content of between 30 and 40% by weight so as to obtain a suspension in water. This suspension is then pregelatinized using a tuyere at the outlet of which a steam counter-pressure is applied which is sufficient to reach a cooking temperature for the suspension of between 125 and 135°C while maintaining an acceptable viscosity so that the flow rate of the milk coming out after cooking is not too low. For example, a counter-pressure of the order of 2 to 3 bar will be applied. Surprisingly and unexpectedly, this cooking temperature is necessary and sufficient to obtain good pregelatinized starch solubility. The amylose fraction exists, according to the process in accordance with the invention, in amorphous form, whereas the prior art processes for cooking amylose-rich starches lead to an amylose which has a high tendency to undergo retro- gradation. The expression "tuyere" is understood to mean any direct steam jet cooking device allowing instant cooking of a starch suspension using pressurized steam. A pregelatinized starch paste is obtained after this cooking, which is then dried on a drum dryer. Such an equipment makes it possible to reproduce, on one and the same device, the cooking and drying stages by exploiting the heat transferred from the surface of the drums heated with steam to the starch paste. Steam pressure values of the order of 2 to 10 bar will be applied, for example, according to the type of starch used. The starch paste is uniformly spread in a thin film over the hot surface of the drums by applying components. The drums are driven in rotation, at a speed of the order of 5 to 8 revolutions per minute. Thus, the cooking of the paste is continued,, followed by drying. The film formed is then scraped using a scraping blade so as to detach a sheet which can then be ground. The process according to the invention makes it possible to homogeneously obtain pregelatinized amylose-rich starches without the need for the use of very high temperatures as taught by the prior art. The process according to the invention is perticularly advantageous because it uses simple techniques, with a lower energy cost than the known techniques of spray- drying or autoclaving. The pregelatinized amylose-rich starches according to the invention are characterized by an apparent density of less than 0.4 g/ml for a mean particle size of 100 micrometres, which is particularly surprising given the higher densities obtained according to the prior art techniques and in particular those described in patent EP-B1 0 366 898. Their solubility in warm water is good, in the region of 80%, whereas it is less than 30% when the tuyere cooking stage is eliminated. These starches have, in addition, various applicative advantages such as, in particular, a good compression capacity, and in particular very good capacities to form a film. This capacity is particularly advantageous for film coating tablets in particular, but also for numerous other applications requiring the formation of a barrier to moisture and to air. To the knowledge of the applicant, such pregelatinized amylose-rich starches capable of having film-forming properties did not exist on the market. The subject of the invention is therefore, in addition, the use of pregelatinized amylose-rich starches for the manufacture of soft gelatin capsules or of hard gelatin capsules, as well as for the coating of solid forms in pharmacy, human foods, animal foods, agrochemistry or plant substances such as seeds. The subject of the invention is also the use of amylose-rich starches obtained according to the invention for the preparation of freshening films, also called flavour sheets. These flavour sheets are small squares of edible films, which are very fine, highly flavoured, and used as breath fresheners by dissolving rapidly in the buccal cavity. The applicant has observed that in addition to the remarkable film- forming properties of the starches according to the invention, the latter had an advantageous capacity to encapsulate molecules with low solubility in water, such as flavourings or certain active ingredients. Indeed, during the formulation of such films based on film-forming polymers, when about 5% of flavouring or of active ingredient which are sparingly soluble in water is added to the film-forming preparation, a total phase separation occurs, during the spreading of the film, between the hydrophobic molecules and the other components. The film-forming solution is pushed to the sides of the band of film, whereas the centre is only composed of flavouring and of active ingredient. The film obtained therefore does not constitute a homogeneous film-coating. The addition, before incorporation of the flavouring, of a pregelatinized amylose-rich starch according to the invention allows, surprisingly and unexpectedly, inclusion of the flavourings or active ingredients which are sparingly soluble in water, on the one hand, and an excellent film quality, on the other hand. Without wishing to be bound to any theory, the applicant is of the opinion that this encapsulation property is linked to the amorphous state of the precooked amylose according to the process in accordance with the invention, given that the precooked amylose-rich starches according to the prior art processes do not possess this encapsulation property. The film obtained has the desired properties, namely good solubility, adequate mechanical properties, strong flavouring and no adherence between each film during packaging. Thus, an edible film which is highly flavoured or which comprises an active ingredient which is sparingly soluble in water, characterized in that it comprises a pregelatinized amylose-rich starch according to the invention, constitutes, to the knowledge of the applicant, a novel industrial product. The expression "sparingly soluble in water" is understood to mean, according to the present invention, flavourings or active ingredients which have a solubility in water of less than 5% by weight. According to a preferred embodiment of the film according to the invention, the latter comprises, on a dry matter basis, 5 to 40%, preferably 5 to 25% of pregelatinized amylose-rich starch according to the invention. According to a still more preferred embodiment of the invention, the said pregelatinized amylose-rich starch is stabilized, for example, by acetylation or hydroxypropylation. The film comprises, in addition, any other film-forming polymer commonly used in practice, such as in particular amylopectin-rich starches, modified or otherwise, amylose-rich starches, modified or otherwise, standard or special maltodextrins, film- forming polysaccharides and proteins such as gelatin, pullulan, plant gums, gluten. According to a preferred variant, the edible film comprises 5 to 40% of pregelatinized amylose-rich starch according to the invention and 40 to 80% of amylopectin-rich starch. The balance for 100% consists of flavourings, active ingredients, sweeteners, one or more humectants and optionally colourings. The final water content of the films according to the invention is generally about 12%. The expression amylopectin-rich starch is understood to mean the so-called waxy starches, derived in particular from maize or potato. According to a still more preferred variant, the said film comprises, on a dry matter basis, 5 to 40%, preferably 5 to 25%, of pregelatinized amylose-rich starch according to the invention, and 40 to 80%, preferably 40 to 70% of waxy starch fluidified by the acid route. A waxy starch derived from maize fluidified by techniques known to persons skilled in the art would be preferably chosen. Of course, the film according to the invention may be used as it is as a flavour sheet for freshening the breath, but it may also be used for the film-coating of various supports, in particular dietary or pharmaceutical supports. There may be mentioned, without limitation, the film-coating of tablets, confectioneries, or any other support. The advantageous properties of encapsulation of substances sparingly soluble in water of the starches according to the invention may also be exploited in any other type of application requiring such properties, in aqueous medium or in the dry state. The invention will be understood more clearly on reading the following examples, which are intended to be explanatory and nonlimiting. Example 1 Amylose-rich starches, modified or otherwise, are prepared according to a process comprising the following steps: - preparation of a suspension of starch and water cooking in a tuyere drying on a drum dryer recovery of a powder In all cases, the initial starch is EURYLON®7 marketed by the applicant, having an amylose content of 70% by weight. The various process parameters are presented in Table 1, as well as the apparent densities and the mean particle sizes of the various products obtained. The apparent density is measured according to the pharmaceutical technical method 2.9.16 of the European Pharmacopoeia, 3rd edition. The mean particle size is calculated from the particle size measured by sieving on successive sieves of 500, 315, 200, 150, 100 and 50 micrometres. The displacement density is measured according to the method described in patent EP-B1 0 366 898. Example 2 In order to illustrate the film-forming properties, the product obtained according to test No. 3 of the preceding example is solubilized in hot water (70- 80°C), with mechanical stirring, at 15% of dry matter. The Brookfield viscosity is 4 000 mPa/s at 70°C and 5 000 mPas s at 60°C. This solution is placed on a polyethylene support over a thickness of 45.7 micrometres. The solution thus deposited is dried at room temperature, and gives a rigid film, which is nonbrittle, and which is insoluble in water. This film can give rise to very numerous applications, since it can serve to coat all types of solid forms which it is desired to protect, whether they are pharmaceutical (tablets, gelatin capsules), dietary (fries, tart bases, confectioneries) or agricultural (seeds, granules). These film-forming properties may also be applied in the manufacture of soft gelatin capsules or hard gelatin capsules. Example 3 Flavour sheets are prepared according to the following procedure: Formula • In a jacketed stainless-steel bowl, disperse the CLEARGUM in a mixture of water, glycerol and saccharinate. Heat to 90°C. • Pour into the bowl of a KENWOOD mixer, add the pregelatinized amylose-rich starch and the flavouring. Mix for 1 minute at the minimum speed (solution S). • Pour the solution S into the stainless-steel bowl and heat to 85°C, degas the mixture as much as possible. • When the mixture is at 85°C, form a film on a plastic plate (thickness of paste = 1.5 mm) with an automatic film applicator (bar-coater B-2105, RK printcoat) equipped with a scale preheated to 60°C. • Allow to dry in an oven at 20°C and 80% relative humidity for 2 days and then end the drying at 20°C under an uncontrolled atmosphere. The film thus obtained, which is highly flavoured, is very soluble, supple and flexible, nonbrittle and not cracked, regular and homogeneous as regards the distribution of the flavour, transparent. It does not stick on contact with other films during prolonged storage. It can therefore be easily used as freshening flavour sheet, or in order to wrap or coat any type of support, in particular a dietary or pharmaceutical support. A film prepared in the same manner but without incorporating starch according to the invention is completely heterogeneous in its centre and impossible to detach from its support in the form of a uniform sheet. WE CLAIM: 1. Process for preparing pregelatinized amylose-rich starch having an amylose content greater than or equal to 50% by weight, characterized in that it comprises the steps consisting of: forming a suspension comprising an amylose-rich starch and water; subjecting the said suspension to steam jet cooking at a temperature between 125°C and 135°C so as to obtain a pregelatinized amylose-rich starch paste; drying the said pregelatinized starch paste on a drum dryer at a pressure between 2 and 10 bar, so as to obtain a pregelatinized amylose-rich starch. 2. Process as claimed in claim 1, wherein, it comprises, in addition, a step for grinding pregelatinized amylose-rich starch, so as to obtain a powder. 3. Process as claimed in either of claims 1 and 2, wherein the amylose content of the said starch is greater than or equal to 50% by weight, and preferably between 50 and 80% by weight. 4. Process as claimed in claim any one of claims 1 to 3, wherein the said starch is a maize starch. 5. Process as claimed in any one of claims 1 to 4, wherein the said suspension has a dry matter content greater than 25% by weight and preferably between 30 and 40% by weight. 6. Process as claimed in any one of claims 1 to 5, wherein the said amylose-rich starch is chemically or physically modified. 7. Process as claim in claim 6, wherein the said modified starch is chosen from the group consisting of acetylated, hydroxypropylated, carboxymethylated and fluidified starches, and starch octenyl succinates. 8. Process as claimed in claim 6, wherein the said modified starch is an acetylated starch. The invention concerns a method for preparing pre-gelatinized starch rich in amylose characterised in that it comprises steps which consist in: forming a suspension comprising a starch rich in amylose and water; subjecting said suspension to a vapour jet cooking at a temperature ranging between 125 and 135°C so as to obtain a starch glue rich in pre-gelatinized amylose; cooking and drying said pre-gelatinized starch glue on a drying drum at a pressure ranging between 2 and 10 bars so as to obtain a pre-gelatinized starch rich in amylose. The invention also concerns a pre-gelatinized starch rich in amylose characterised in that it has an apparent density less than 0.4g/ml for an average grain size distribution of 100 micrometers. The invention further concerns such a starch for making soft capsules or tablets and film-coating of solid pharmaceutical, food or agricultural formulations.

Full Text

The subject of the invention is a novel process for
preparing pregelatinized amylose-rich starches.
Its subject is also the starches obtained by this
process.
Pregelatinized starches are generally prepared by
thermal, chemical or mechanical techniques which can
cause swelling of the starch granules so that they are
soluble in cold water.
The preferred techniques are spray-drying, cooking on a
drum or extrusion. Autoclaving or indirect heating on a
heat exchanger are cooking processes which tend to
produce complex colloidal dispersions consisting of
intact, fragmented and swollen granules.
It is well known that amylose-rich starches, that is to
say which have more than 50% by weight of amylose, are
particularly difficult to disperse and require high
cooking temperatures.
The document US-A-3 086 890 describes a process for
preparing pregelatinized amylose. This process consists
in autoclaving at 191°C, under pressure, a solution of
amylose containing at most 25% by weight of dry matter,
and then drum-drying at 110-200°C. The powders obtained
are amorphous and form irreversible gels after
dispersion. Their apparent density is high, that is to
say generally greater than 0.4 g/ml.
The document US-A-3 607 394 describes a process for the
pregelatinization of starches having amylose contents
of less than 60% by weight. This process consists in
cooking the starch at 149°C, followed by drum-drying,
spray-drying or another type of drying means.
The document EP 0 366 898 describes a coupled cooking/
spray-drying process which makes it possible to obtain
amorphous products, which are practically free of
retrogradation, and which have an apparent density
greater than that of an identical starch which has been
subjected to the same process but in two separate
stages, that is an apparent density greater than
0.45 g/ml. The cooking of amylose-rich starches is
carried out on a jet cooker at 143°C and the spray-
drying is carried out with an inlet air temperature of
220°C. This document presents, in Figure 7, a
comparison of various prior art pregelatinized
starches.
Starting from this teaching, the applicant has now
found, after long research studies, that it was
possible to prepare a pregelatinized amylose-rich
starch using a particular process leading to products
of low apparent density while working at not very high
temperatures, which none of the prior art techniques
made it possible to obtain.
The subject of the invention is therefore a process for
preparing pregelatinized amylose-rich starch,
characterized in that it comprises the steps consisting
in:
forming a suspension comprising an amylose-rich
starch and water;
subjecting the said suspension to steam jet
cooking at a temperature of between 125 and
135°C so as to obtain a pregelatinized amylose-
rich starch paste;
- drying the said pregelatinized starch on a drum
dryer at a pressure of between 2 and 10 bar, so
as to obtain a pregelatinized amylose-rich
starch.
The pregelatinized amylose-rich starch obtained may
then be recovered and ground so as to obtain a powder
having a particle size which is chosen according to the
uses which will be subsequently made thereof.
The expression "amylose-rich starches" according for
the purposes of the present invention denotes starches
having an amylose content greater than or equal to 50%
by weight, and preferably of between 50 and 80% by
weight, obtained from any plant origin, such as in
particular maize, potato, cassava.
Preferably, the process according to the invention uses
a maize starch such as, for example, EURYLON® marketed
by the applicant.
The invention also applies to chemically or physically
modified amylose-rich starches. Preferably, the
modified starch will be chosen from the group
consisting of acetylated, hydroxypropylated, carboxy-
methylated and fluidified starches, and starch octenyl
succinates.
According to a preferred variant of the process
according to the invention, an acetylated starch will
be chosen.
The starch suspension is prepared at a dry matter
content of between 30 and 40% by weight so as to obtain
a suspension in water.
This suspension is then pregelatinized using a tuyere
at the outlet of which a steam counter-pressure is
applied which is sufficient to reach a cooking
temperature for the suspension of between 125 and 135°C
while maintaining an acceptable viscosity so that the
flow rate of the milk coming out after cooking is not
too low. For example, a counter-pressure of the order
of 2 to 3 bar will be applied.
Surprisingly and unexpectedly, this cooking temperature
is necessary and sufficient to obtain good
pregelatinized starch solubility. The amylose fraction
exists, according to the process in accordance with the
invention, in amorphous form, whereas the prior art
processes for cooking amylose-rich starches lead to an
amylose which has a high tendency to undergo retro-
gradation.
The expression "tuyere" is understood to mean any
direct steam jet cooking device allowing instant
cooking of a starch suspension using pressurized steam.
A pregelatinized starch paste is obtained after this
cooking, which is then dried on a drum dryer.
Such an equipment makes it possible to reproduce, on
one and the same device, the cooking and drying stages
by exploiting the heat transferred from the surface of
the drums heated with steam to the starch paste. Steam
pressure values of the order of 2 to 10 bar will be
applied, for example, according to the type of starch
used. The starch paste is uniformly spread in a thin
film over the hot surface of the drums by applying
components. The drums are driven in rotation, at a
speed of the order of 5 to 8 revolutions per minute.
Thus, the cooking of the paste is continued,, followed
by drying. The film formed is then scraped using a
scraping blade so as to detach a sheet which can then
be ground.
The process according to the invention makes it
possible to homogeneously obtain pregelatinized
amylose-rich starches without the need for the use of
very high temperatures as taught by the prior art. The
process according to the invention is perticularly
advantageous because it uses simple techniques, with a
lower energy cost than the known techniques of spray-
drying or autoclaving.
The pregelatinized amylose-rich starches according to
the invention are characterized by an apparent density
of less than 0.4 g/ml for a mean particle size of
100 micrometres, which is particularly surprising given
the higher densities obtained according to the prior
art techniques and in particular those described in
patent EP-B1 0 366 898.
Their solubility in warm water is good, in the region
of 80%, whereas it is less than 30% when the tuyere
cooking stage is eliminated.
These starches have, in addition, various applicative
advantages such as, in particular, a good compression
capacity, and in particular very good capacities to
form a film. This capacity is particularly advantageous
for film coating tablets in particular, but also for
numerous other applications requiring the formation of
a barrier to moisture and to air. To the knowledge of
the applicant, such pregelatinized amylose-rich
starches capable of having film-forming properties did
not exist on the market. The subject of the invention
is therefore, in addition, the use of pregelatinized
amylose-rich starches for the manufacture of soft
gelatin capsules or of hard gelatin capsules, as well
as for the coating of solid forms in pharmacy, human
foods, animal foods, agrochemistry or plant substances
such as seeds.
The subject of the invention is also the use of
amylose-rich starches obtained according to the
invention for the preparation of freshening films, also
called flavour sheets. These flavour sheets are small
squares of edible films, which are very fine, highly
flavoured, and used as breath fresheners by dissolving
rapidly in the buccal cavity. The applicant has
observed that in addition to the remarkable film-
forming properties of the starches according to the
invention, the latter had an advantageous capacity to
encapsulate molecules with low solubility in water,
such as flavourings or certain active ingredients.
Indeed, during the formulation of such films based on
film-forming polymers, when about 5% of flavouring or
of active ingredient which are sparingly soluble in
water is added to the film-forming preparation, a total
phase separation occurs, during the spreading of the
film, between the hydrophobic molecules and the other
components. The film-forming solution is pushed to the
sides of the band of film, whereas the centre is only
composed of flavouring and of active ingredient. The
film obtained therefore does not constitute a
homogeneous film-coating. The addition, before
incorporation of the flavouring, of a pregelatinized
amylose-rich starch according to the invention allows,
surprisingly and unexpectedly, inclusion of the
flavourings or active ingredients which are sparingly
soluble in water, on the one hand, and an excellent
film quality, on the other hand. Without wishing to be
bound to any theory, the applicant is of the opinion
that this encapsulation property is linked to the
amorphous state of the precooked amylose according to
the process in accordance with the invention, given
that the precooked amylose-rich starches according to
the prior art processes do not possess this
encapsulation property. The film obtained has the
desired properties, namely good solubility, adequate
mechanical properties, strong flavouring and no
adherence between each film during packaging.
Thus, an edible film which is highly flavoured or which
comprises an active ingredient which is sparingly
soluble in water, characterized in that it comprises a
pregelatinized amylose-rich starch according to the
invention, constitutes, to the knowledge of the
applicant, a novel industrial product. The expression
"sparingly soluble in water" is understood to mean,
according to the present invention, flavourings or
active ingredients which have a solubility in water of
less than 5% by weight.
According to a preferred embodiment of the film
according to the invention, the latter comprises, on a
dry matter basis, 5 to 40%, preferably 5 to 25% of
pregelatinized amylose-rich starch according to the
invention. According to a still more preferred
embodiment of the invention, the said pregelatinized
amylose-rich starch is stabilized, for example, by
acetylation or hydroxypropylation.
The film comprises, in addition, any other film-forming
polymer commonly used in practice, such as in
particular amylopectin-rich starches, modified or
otherwise, amylose-rich starches, modified or
otherwise, standard or special maltodextrins, film-
forming polysaccharides and proteins such as gelatin,
pullulan, plant gums, gluten.
According to a preferred variant, the edible film
comprises 5 to 40% of pregelatinized amylose-rich
starch according to the invention and 40 to 80% of
amylopectin-rich starch. The balance for 100% consists
of flavourings, active ingredients, sweeteners, one or
more humectants and optionally colourings. The final
water content of the films according to the invention
is generally about 12%.
The expression amylopectin-rich starch is understood to
mean the so-called waxy starches, derived in particular
from maize or potato.
According to a still more preferred variant, the said
film comprises, on a dry matter basis, 5 to 40%,
preferably 5 to 25%, of pregelatinized amylose-rich
starch according to the invention, and 40 to 80%,
preferably 40 to 70% of waxy starch fluidified by the
acid route.
A waxy starch derived from maize fluidified by
techniques known to persons skilled in the art would be
preferably chosen.
Of course, the film according to the invention may be
used as it is as a flavour sheet for freshening the
breath, but it may also be used for the film-coating of
various supports, in particular dietary or
pharmaceutical supports. There may be mentioned,
without limitation, the film-coating of tablets,
confectioneries, or any other support.
The advantageous properties of encapsulation of
substances sparingly soluble in water of the starches
according to the invention may also be exploited in any
other type of application requiring such properties, in
aqueous medium or in the dry state.
The invention will be understood more clearly on
reading the following examples, which are intended to
be explanatory and nonlimiting.
Example 1
Amylose-rich starches, modified or otherwise, are
prepared according to a process comprising the
following steps:
- preparation of a suspension of starch and water
cooking in a tuyere
drying on a drum dryer
recovery of a powder
In all cases, the initial starch is EURYLON®7 marketed
by the applicant, having an amylose content of 70% by
weight.
The various process parameters are presented in
Table 1, as well as the apparent densities and the mean
particle sizes of the various products obtained. The
apparent density is measured according to the
pharmaceutical technical method 2.9.16 of the European
Pharmacopoeia, 3rd edition. The mean particle size is
calculated from the particle size measured by sieving
on successive sieves of 500, 315, 200, 150, 100 and
50 micrometres.
The displacement density is measured according to the
method described in patent EP-B1 0 366 898.
Example 2
In order to illustrate the film-forming properties, the
product obtained according to test No. 3 of the
preceding example is solubilized in hot water (70-
80°C), with mechanical stirring, at 15% of dry matter.
The Brookfield viscosity is 4 000 mPa/s at 70°C and
5 000 mPas s at 60°C.
This solution is placed on a polyethylene support over
a thickness of 45.7 micrometres.
The solution thus deposited is dried at room
temperature, and gives a rigid film, which is
nonbrittle, and which is insoluble in water.
This film can give rise to very numerous applications,
since it can serve to coat all types of solid forms
which it is desired to protect, whether they are
pharmaceutical (tablets, gelatin capsules), dietary
(fries, tart bases, confectioneries) or agricultural
(seeds, granules).
These film-forming properties may also be applied in
the manufacture of soft gelatin capsules or hard
gelatin capsules.
Example 3
Flavour sheets are prepared according to the following
procedure:
Formula
• In a jacketed stainless-steel bowl, disperse the
CLEARGUM in a mixture of water, glycerol and
saccharinate. Heat to 90°C.
• Pour into the bowl of a KENWOOD mixer, add the
pregelatinized amylose-rich starch and the
flavouring. Mix for 1 minute at the minimum
speed (solution S).
• Pour the solution S into the stainless-steel
bowl and heat to 85°C, degas the mixture as much
as possible.
• When the mixture is at 85°C, form a film on a
plastic plate (thickness of paste = 1.5 mm) with
an automatic film applicator (bar-coater B-2105,
RK printcoat) equipped with a scale preheated to
60°C.
• Allow to dry in an oven at 20°C and 80% relative
humidity for 2 days and then end the drying at
20°C under an uncontrolled atmosphere.
The film thus obtained, which is highly flavoured, is
very soluble, supple and flexible, nonbrittle and not
cracked, regular and homogeneous as regards the
distribution of the flavour, transparent. It does not
stick on contact with other films during prolonged
storage. It can therefore be easily used as freshening
flavour sheet, or in order to wrap or coat any type of
support, in particular a dietary or pharmaceutical
support.
A film prepared in the same manner but without
incorporating starch according to the invention is
completely heterogeneous in its centre and impossible
to detach from its support in the form of a uniform
sheet.
WE CLAIM:
1. Process for preparing pregelatinized amylose-rich starch having an
amylose content greater than or equal to 50% by weight,
characterized in that it comprises the steps consisting of:
forming a suspension comprising an amylose-rich starch and
water;
subjecting the said suspension to steam jet cooking at a
temperature between 125°C and 135°C so as to obtain a
pregelatinized amylose-rich starch paste;
drying the said pregelatinized starch paste on a drum dryer at a
pressure between 2 and 10 bar, so as to obtain a pregelatinized
amylose-rich starch.
2. Process as claimed in claim 1, wherein, it comprises, in addition, a
step for grinding pregelatinized amylose-rich starch, so as to obtain a
powder.
3. Process as claimed in either of claims 1 and 2, wherein the amylose
content of the said starch is greater than or equal to 50% by weight,
and preferably between 50 and 80% by weight.
4. Process as claimed in claim any one of claims 1 to 3, wherein the said
starch is a maize starch.
5. Process as claimed in any one of claims 1 to 4, wherein the said
suspension has a dry matter content greater than 25% by weight and
preferably between 30 and 40% by weight.
6. Process as claimed in any one of claims 1 to 5, wherein the said
amylose-rich starch is chemically or physically modified.
7. Process as claim in claim 6, wherein the said modified starch is
chosen from the group consisting of acetylated, hydroxypropylated,
carboxymethylated and fluidified starches, and starch octenyl
succinates.
8. Process as claimed in claim 6, wherein the said modified starch is an
acetylated starch.
The invention concerns a method for preparing pre-gelatinized starch rich in
amylose characterised in that it comprises steps which consist in: forming a suspension
comprising a starch rich in amylose and water; subjecting said suspension to a vapour jet
cooking at a temperature ranging between 125 and 135°C so as to obtain a starch glue
rich in pre-gelatinized amylose; cooking and drying said pre-gelatinized starch glue on a
drying drum at a pressure ranging between 2 and 10 bars so as to obtain a pre-gelatinized
starch rich in amylose. The invention also concerns a pre-gelatinized starch rich in
amylose characterised in that it has an apparent density less than 0.4g/ml for an average
grain size distribution of 100 micrometers. The invention further concerns such a starch
for making soft capsules or tablets and film-coating of solid pharmaceutical, food or
agricultural formulations.

Documents:

« Previous Patent

Next Patent »

Patent Number

224208

Indian Patent Application Number

IN/PCT/2002/01445/KOL

PG Journal Number

41/2008

Publication Date

10-Oct-2008

Grant Date

03-Oct-2008

Date of Filing

25-Nov-2002

Name of Patentee

ROQUETTE FRERES

Applicant Address

62136 LESTREM

Inventors:

#	Inventor's Name	Inventor's Address
1	CARBONE DOMENICO	VIA ROMA, 21 15060 PASTURANA (AL)
2	QUETTIER CLAUDE	7, RUE DE STADE, 59193 ERQUINGHEM LYS
3	SEMINO GIOVANNI	REGIONE POGGIO, 14, 15063 CASSANO SPINOLA (AL)
4	FOSSATI ERNESTO	VIA DOGANA, 8/3, 15067 NOVI LIGURE (AL)

PCT International Classification Number

C08B 30/14

PCT International Application Number

PCT/FR02/01031

PCT International Filing date

2002-03-25

PCT Conventions:

#	PCT Application Number	Date of Convention	Priority Country
1	01/04,023	2001-03-26	France